US7906095B2 - Method of growing carbon nanotube and carbon nanotube growing system - Google Patents
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- US7906095B2 US7906095B2 US12/146,841 US14684108A US7906095B2 US 7906095 B2 US7906095 B2 US 7906095B2 US 14684108 A US14684108 A US 14684108A US 7906095 B2 US7906095 B2 US 7906095B2
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
- H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
- H01L21/76838—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the conductors
- H01L21/76877—Filling of holes, grooves or trenches, e.g. vias, with conductive material
- H01L21/76879—Filling of holes, grooves or trenches, e.g. vias, with conductive material by selective deposition of conductive material in the vias, e.g. selective C.V.D. on semiconductor material, plating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
- C01B32/162—Preparation characterised by catalysts
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
- H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
- H01L21/285—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation
- H01L21/28506—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers
- H01L21/28512—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic System
- H01L21/28556—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic System by chemical means, e.g. CVD, LPCVD, PECVD, laser CVD
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/52—Arrangements for conducting electric current within the device in operation from one component to another, i.e. interconnections, e.g. wires, lead frames
- H01L23/522—Arrangements for conducting electric current within the device in operation from one component to another, i.e. interconnections, e.g. wires, lead frames including external interconnections consisting of a multilayer structure of conductive and insulating layers inseparably formed on the semiconductor body
- H01L23/532—Arrangements for conducting electric current within the device in operation from one component to another, i.e. interconnections, e.g. wires, lead frames including external interconnections consisting of a multilayer structure of conductive and insulating layers inseparably formed on the semiconductor body characterised by the materials
- H01L23/53204—Conductive materials
- H01L23/53276—Conductive materials containing carbon, e.g. fullerenes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2221/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof covered by H01L21/00
- H01L2221/10—Applying interconnections to be used for carrying current between separate components within a device
- H01L2221/1068—Formation and after-treatment of conductors
- H01L2221/1094—Conducting structures comprising nanotubes or nanowires
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
- H01L2924/0001—Technical content checked by a classifier
- H01L2924/0002—Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00
Definitions
- the present invention relates to a method of growing a carbon nanotube and a carbon nanotube growing system.
- a catalytic metal thin film is formed by a sputtering method or a vapor deposition method, and thereafter, the catalytic metal thin film is heated while introducing a reduction gas or an inert gas into a chamber, to thereby make the catalytic metal thin film be fine particles (For example, see Japanese Patent Application Laid-open Nos. 2004-267926 and 2002-530805).
- a raw gas such as acetylene gas starts to be supplied into a chamber, and with the use of a thermal CVD method, a plasma CVD method, a hot filament CVD method or the like, the carbon nanotubes are grown.
- a manufacturing method of carbon nanotubes according to an aspect of the present invention comprises: adhering catalytic particles to an upper surface of a substrate; and raising a substrate temperature at a speed of 500° C./minute or faster in a chamber with a raw gas containing carbon atoms previously introduced therein.
- a carbon nanotube growing system is provided with a catalyst adhering portion adhering catalytic particles to an upper surface of a substrate, and a thermal treatment portion raising a substrate temperature at a speed of 500° C./minute or faster in a chamber with a raw gas containing carbon atoms previously introduced therein.
- FIG. 1A is a sectional view showing a method of growing carbon nanotubes according to a first embodiment
- FIG. 1B is a sectional view showing the method of growing carbon nanotubes following FIG. 1A ;
- FIG. 1C is a sectional view showing the method of growing carbon nanotubes following FIG. 1B ;
- FIG. 1D is a sectional view showing the method of growing carbon nanotubes following FIG. 1C ;
- FIG. 1E is a sectional view showing the method of growing carbon nanotubes following FIG. 1D ;
- FIG. 1F is a sectional view showing the method of growing carbon nanotubes following FIG. 1E ;
- FIG. 2 is a view showing a temperature control in the first embodiment
- FIG. 3 is a view showing details of carbon nanotubes 17 ;
- FIG. 4 is a view showing an example of a temperature control
- FIG. 5A is a SEM micrograph showing carbon nanotubes grown based on an example No. 1;
- FIG. 5B is a view schematically showing the carbon nanotubes grown based on the example No. 1;
- FIG. 6A is an SEM micrograph showing carbon nanotubes grown based on an example No. 2;
- FIG. 6B is a view schematically showing the carbon nanotubes grown based on the example No. 2;
- FIG. 7A is an SEM micrograph showing carbon nanotubes grown based on an example No. 3;
- FIG. 7B is a view schematically showing the carbon nanotubes grown based on the example No. 3;
- FIG. 8 is a view showing a temperature control in the example No. 3;
- FIG. 9A is a sectional view showing a method of growing carbon nanotubes according to a second embodiment
- FIG. 9B is a sectional view showing the method of growing carbon nanotubes following FIG. 9A ;
- FIG. 9C is a sectional view showing the method of growing carbon nanotubes following FIG. 9B ;
- FIG. 9D is a sectional view showing the method of growing carbon nanotubes following FIG. 9C ;
- FIG. 10A is a view showing another example of a temperature control
- FIG. 10B is a view showing further another example of a temperature control.
- FIG. 11 is a view showing an example of a temperature control and an atmosphere control.
- FIGS. 1A to 1F are sectional views showing a method of growing carbon nanotubes according to the first embodiment in order of step.
- a silicon oxide (SiO 2 ) film 12 is formed on a silicon (Si) substrate 11 , as shown in FIG. 1A .
- a thickness of the silicon oxide (SiO 2 ) film 12 is, for example, about 350 nm.
- a resist pattern 13 having a circular opening portion 13 a is formed on the silicon oxide (SiO 2 ) film 12 .
- the opening portion 13 a has a diameter of, for example, about 2 ⁇ m.
- the silicon oxide (SiO 2 ) film 12 is patterned using the resist pattern 13 .
- a cylindrical opening portion 14 is formed in the silicon oxide (SiO 2 ) film 12 , as shown in FIG. 1B .
- a catalytic layer 15 is formed at a bottom portion of the opening portion 14 , as shown in FIG. 1C .
- a titanium (Ti) film having about 1 nm in thickness, for example, is formed.
- the catalytic particle 16 has a diameter of, for example, 5 nm or smaller.
- As the catalytic particles 16 cobalt (Co) particles, nickel (Ni) particles, or iron (Fe) particles are used, for example. It should be noted that alloy particles of these elements may also be used.
- the catalytic particles 16 may adhere on the resist pattern 13 , as shown in FIG. 1D .
- a method for adhering the catalytic particles 16 is not limited in particular. For example, a method described in Japanese Patent Application Laid-open No. 2005-22886 may be applied.
- the resist pattern 13 is removed by ashing or the like, as shown in FIG. 1E .
- the catalytic particles 16 are removed.
- carbon nanotubes 17 are grown from the catalytic particles 16 on the catalytic layer 15 , as shown in FIG. 1F .
- the silicon (Si) substrate 11 on which the catalytic layer 15 is formed is delivered into a thermal CVD chamber (not shown) whose internal temperature is, for example, a room temperature (R.T.), and a mixed gas of an inert gas and a raw gas is introduced into the inside thereof.
- a mixed gas in which a raw gas (acetylene gas) is diluted by an inert gas (argon gas) is used. Then, after the pressure inside of the chamber is stabilized at 1 kPa, for example, the temperature inside of the chamber is raised to 510° C. in 1 minute, as shown in FIG. 2 . As a result, the carbon nanotubes 17 start to grow linearly from the respective catalytic particles 16 without any fusion of each of the catalytic particles 16 .
- the temperature and an atmosphere are maintained for about 30 minutes, for example.
- the carbon nanotubes 17 start to grow, surfaces of the catalytic particles 16 are covered by carbon, so that any fusion of each of the catalytic particles 16 can be avoided even during the maintenance for about 30 minutes.
- the temperature is lowered to the room temperature, while keeping the atmosphere.
- the carbon nanotubes 17 initiate the growth immediately from the start of the heating. Therefore, the catalytic particles 16 do not fuse together, as described above. Further, since the temperature is raised at high speed, the fusion of each of the catalytic particles 16 can be prevented further securely. As a result, the diameter of the carbon nanotube 17 is determined depending on the diameter of the adhered catalytic particle 16 . Further, the present embodiment applies the catalytic particles 16 having the substantially uniform diameters (about 5 nm, for example), so that a variation of the diameters of the carbon nanotubes 17 grown from the catalytic particles 16 also becomes extremely small.
- the carbon nanotube 17 which is grown according to the above-described embodiment includes a straight portion 17 a and a crimped portion 17 b , as shown in FIG. 3 .
- the carbon nanotube 17 grows linearly when raising a temperature at high speed, but it grows while being crimped when maintaining the temperature.
- the straight portion 17 a has smaller defects and lower resistance values. Therefore, it is preferable to select a condition under which the straight portion 17 a grows longer. According to the results of experiments performed so far by the present inventor, it is favorable to set the pressure inside of the chamber at 0.1 kPa to 30 kPa, and the speed of raising the temperature at 500° C./minute or faster, for example.
- the period of time taken for raising the temperature is also not limited in particular, and it is set at, for example, more than 30 seconds or more than 1 minute.
- the temperature to be achieved by the high-speed temperature rise may be the one at which the carbon nanotubes can grow, and is set at, for example, 400° C. or higher.
- the temperature to be maintained thereafter may also be the one at which the carbon nanotubes can grow.
- the temperature is preferable to be set at 450° C. or lower.
- the raw gas is not limited to the acetylene gas, and various hydrocarbon gases can also be applied.
- the catalytic particles may contain titanium (Ti), molybdenum (Mo), palladium (Pd), tantalum (Ta), aluminum (Al), tungsten (W), copper (Cu), vanadium (V), hafnium (Hf) and/or zirconium (Zr), in addition to iron (Fe), cobalt (Co) and/or nickel (Ni).
- Ti titanium
- Mo molybdenum
- Pd palladium
- Ta tantalum
- Al aluminum
- Cu copper
- vanadium (V) hafnium (Hf) and/or zirconium (Zr) in addition to iron (Fe), cobalt (Co) and/or nickel (Ni).
- the temperature may be maintained between the periods of raising the temperature at high speed and lowering the temperature, as shown in FIG. 10B .
- the carbon nanotubes can also be grown by performing a control as shown in FIG. 11 .
- a temperature is raised at high speed to 510° C. in 1 minute in a mixed gas (1 kPa) of acetylene (C 2 H 2 ) and argon (Ar).
- the carbon nanotubes are grown from almost all of the catalytic fine particles, but, there exists some from which the carbon nanotubes are not grown. This is because the catalytic fine particles are covered by carbon before the carbon nanotubes start to grow therefrom.
- the raw gas is once evacuated and oxygen is newly introduced into the chamber until the pressure in the chamber reaches 1 kPa.
- the temperature is raised at high speed from the room temperature to 510° C. in 1 minute in the oxygen atmosphere. By conducting this process, the carbon covering the catalytic fine particles is removed.
- the temperature is lowered to the room temperature, and again, the temperature is raised at high speed to 510° C. in 1 minute in the mixed gas (1 kPa) of acetylene and argon.
- the carbon nanotubes are grown from almost all of the catalytic fine particles from which the carbon nanotubes are not grown at the first time of the high-speed temperature rise.
- the carbon nanotubes can be grown from almost all of the catalytic fine particles. As a result, it becomes possible to obtain the carbon nanotubes grown in high density that may not be obtained at one time of the high-speed temperature rise. Note that, a condition(s) under which the temperature is raised at high speed and/or the oxidation is performed for the second time or thereafter may vary from that (those) of the first time.
- a unit adhering catalysts (catalyst adhering portion) and a thermal treatment unit performing the high-speed temperature rise (thermal treatment portion) and the like may be provided separately or in combination.
- FIG. 5A , FIG. 6A and FIG. 7A contents of the SEM micrographs shown in FIG. 5A , FIG. 6A and FIG. 7A , respectively, are schematically shown in FIG. 5B , FIG. 6B and FIG. 7B .
- the carbon nanotubes shown in FIG. 5A and FIG. 5B were grown based on a method according to the above-described embodiment (example No. 1).
- the carbon nanotubes shown in FIG. 6A and FIG. 6B were grown based on a method according to the above-described embodiment in which a pressure in the chamber was changed (example No. 2). In the example No.
- the pressure in the chamber was set at 10 kPa.
- the carbon nanotubes shown in FIG. 7A and FIG. 7B were grown based on a method according to the above-described embodiment in which a temperature control was changed (example No. 3).
- the temperature in the chamber was raised to 510° C. in 30 minutes, as shown in FIG. 8 .
- FIGS. 9A to 9D are sectional views showing a method of growing carbon nanotubes according to the second embodiment in order of step.
- a silicon oxide (SiO 2 ) film 22 is formed on a silicon (Si) substrate 21 , as shown in FIG. 9A .
- a thickness of the silicon oxide (SiO 2 ) film 22 is, for example, about 350 nm.
- a catalytic layer 25 is formed on the silicon oxide (SiO 2 ) film 22 , as shown in FIG. 9B .
- the catalytic particle 26 has a diameter of, for example, 5 nm or smaller.
- As the catalytic particles 26 cobalt (Co) particles, nickel (Ni) particles, or iron (Fe) particles are used, for example. Further, alloy particles of these elements may also be used.
- a method for adhering the catalytic particles 26 is not limited in particular. For example, the method described in Japanese Patent Application Laid-open No. 2005-22886 may be applied, similar to the first embodiment.
- carbon nanotubes 27 are grown from the catalytic particles 26 on the catalytic layer 25 , as shown in FIG. 9D .
- the carbon nanotubes 27 can be grown using a similar method as is used for growing the carbon nanotubes 17 in the first embodiment.
Abstract
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US13/022,110 US8501108B2 (en) | 2005-12-26 | 2011-02-07 | Carbon nanotube growing system |
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PCT/JP2005/023799 WO2007074506A1 (en) | 2005-12-26 | 2005-12-26 | Method of growing carbon nanotube and carbon nanotube growing system |
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WO2007074506A1 (en) | 2007-07-05 |
JPWO2007074506A1 (en) | 2009-06-04 |
US20080260618A1 (en) | 2008-10-23 |
US8501108B2 (en) | 2013-08-06 |
US20110142727A1 (en) | 2011-06-16 |
JP4924433B2 (en) | 2012-04-25 |
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